Method of producing nitrogen compounds from carbids.



A. R. FRANK. METHOD OF PRODUCING NITROGEN COMPOUNDS FROM OARBIDS. APPLICATION FILED MAR. 13, 1907.

Patented OCE. 24, 1911,

bythe.

`ALBERT R. FRANK, OF HALENSEE, NEAR BERLIN, GERMANY, ASSIG-NOR T O SOCIET GENERALE PEB LA CIANAMIDE, OF ROME, ITALY, A CORPORATION 0F ITALY.

METHOD 0F PRODUCING NITROGEN COMPOUNDS FIB/OM CARBIDS.4

Speciycation of Letters Patent. Patented Oct,

Application filed March 13, 1907. Serial No. 362,986.

`compounds, as applied to the production of which the process would be illustrated by the formulae i In the production of nitrogen compounds tion of. nitrogen with carbids, as i for example, the carbids of the alkalis or alkaline earths, it has been ascertained that it is not necessary for the process that the entire mass of the carbid be brought to the temperature necessary for the reaction; but that it vsuffices if this temperature be produced at one place in the mass, the reaction then proceeding or continuing, under suitable condit-ions of nitrogen supply, spontaneously throughout the entire mass; a preliminary condition however is that the reaction temperature be actually attained at this one place.

In accordancewith the present invention the process may be carried out in several ways, of which the following lare examples: The ignition at one place may be produced by any convenient form of igniterwhich will raise the temperature at that place to the temperature of the reaction, that is to say to a temperature lying between about 800o to 1100o C., whereupon the reaction will proceed without the application of further heat.

The ignition may be accomplished, for example, by means of an electric heater or resistor in the form of a carbon body, or a' metallic conductor or semi-conductor lplaced i in a heat-insulated receptacle containing the f carbid. The heater is then raised to-or above' the reaction temperature by turning on the 5 electric current. The nitrogen bein brought 'finto contact with the carbid in t e receptacle, the reaction proceeds from. the region ,of the heater until the entire mass of the carbid is converted in to the desired nitrogen compound. If the heat insulation of the reg ceptacle be sufficient-ly effective, the current l may be switched oil after the reaction has commenced; but if said insulation be not suiiiciently effective, heat may be applied,

through the resistor or otherwise, during the entire period of the reaction to compensate for the loss of heat. As an illustration of one method of carry- Y ing out my invention, I will select the ro- Q duction of calcium cyanamid (CaCN2) rom .,1 calcium carbid ('CaC2) and nitrogen (N),

5 following the reaction,

CaC2|2N=CaCN2+C,'

i which may be carried out as follows: Into a suitable receptacle, (preferably closed) con- 1 structed of material of low heat conductivity, provided with means for introducing nitrogen and containing electrical vmeans of 'developing a temperature lying between 4dark red and light yellow, I introduce the desired quantity, say 100 k. g., of finely divided calcium lcarbid. A small portion ofthe carbid immediately adjacent to the electrical heat-developing means, is first raised to the temperature required to initiate the reaction at that point, between thecarbid and the nitrogen then or previously introduced, and the process of conversion starts. The supply of nitrogen being maintained, the heat spontaneously resulting from the reaction between the4 carbid and nitrogen at this initial stage which we may call the ignition stage of the process is transmitted to that portion of the mass immediately surrounding the initially heated portion, and is suflicient to promotethe reaction in said surrounding portion and there develop a new supply of heat, which,

transmitted tov an area still more remote from the ignition point is suiicient to'p'og forming e part of this specification. in

' temperature of reaction when nitr 'cete on carbide,

inotethe reaction there; and so the rer' continues to spread until conversion o ciuin carbid into calcium cynnurnid is enecithroughout the entire mos'e. dilisis rf; Wili be recognized from the cessation in consumption of nitrogen, which may be served in any Weil known manner.

Referring t the accompanying dra.

the figure is e diagrammatic sectioned vien`r ci.' en apparatus suitable :tor cari ff i this invention, a; represents any suit ceptncle, the material to be acted iu nitrogen, o any Suitable means tor ne seid meterial, for exe-mpio, through which e, urren "nay ine' pesi, the positive terminal of c 'wordt f the negative terminai; i e tube or ot" ceptacle through which the resistor c pass and j" any suitooe closur s receptacle.

f The invention may also 19e carrbringing the carbid reduced to if; vided. state, end either cold or ined l heated, into contact with higliiy in ed trogen; underv these conditions the f becomes incandescent and reacts i nitrogen, the supply of which is nieir f the procese proceeding as loe-fore de The nitrogen may also be er i sure alcove tliet of the mospheric pressure, or it ine the rccepteclexat the atmosphere.

iin all Ceses the carbide may loe ein either in. the pure state or es conv clci carbide or mixed with other materiele., ticuleriy with suoli materiels es eiiect loosening of the cerbic'` mess, such, for instence',"es cerbonaceous rneteriais winch oy becoming cerloonized orxn channels or pores in the mass, which channeis or pores eneide the nitrogen to penetrate readily and vcoinpleteiy all the portions of the mess. The carbid muy oe employed either in the pow-- dered state or liiroren into lumps. Further, carbid einpioyed need not be completely formed carbid but may be employed in 'the forni of its components, es, for exemple, e, mixture' of oxide, cerbonetes or other Seite of elkelis or alkaline certhe and carbon or any cerooneceous gunst-ences; or e n turevof ineteis und carbon'or substnnce lived 'from carbon with or 'Without the e dition oit" other organic or inorganic sui;- stencee, provided these componente do not contain compounds hay ng a. temperature of decomposition which iii itseif or in reectiin with thc-.ether components liiflier if 'be draft-rn i pressure beton" tlm...

the carbid mass only lall pure carbide as such but also carbide in the forni o thenl components, such as a mixture of oxide or other salts or metals with cnrooneceous materiel, as indicated above.

empemturc of reaction when nitrogen acts on carbid,

ift is also to be understood that the word nitrosclgen'w es used in this specitcaition end in the cieims species and inciudes not only pure nitrogen es such, but nitrogen mixed 1 other gases, vapors or substances and mogen in the combined state, as ammonia, for exemple. I

en; that nitrogen compounds have hitherto been produced rom'carbids by the action of nitrogen. upon carbide and l therefore do not cieiin such method or process broadly, 'but The process of making compounds of "i'og'en by reacting on carbide with nitront e euitabie temperature, Whicliconsiste in lien-ting; e Yetiveiy smc-ii part of the ceilid niece ing; temperature, supreaction proceeds,

continuing the reaction throughout J to be converted.

The process of making compounds of nitrogen by reacting on carbide With nitroa, suitable temperature, which conin initiating the process by physically heating relatively small part of the carbid mess to a reacting temperature, supplying nitrogen as' the `reaction proceeds, thereby maintaining the temperature and continuinfg" the reaction throughout the mess to be converted.

3. The process of making compounds of nitrogen by reacting on cerbids with nitrogen 'et e suitable temperature, which consists in bringing a relatively smell part of in a. finely divided condition into contact with heated nitrogen to neet seid carbid supplying nitrogen es the reaction proceeds, thereby maintaining the temperature and continuing the reaction throughout the mass to 'be converted. A

fl; The process of mekinn compounds of nitrogen by reacting on car ids with nitrogen a suite-ole temperature, which sconin heating a reietiveiy small part of the carbid nui-es to e reacting temperature, suipiying nitrogen :it e pressure above that ot the atmosphere as the reaction proceeds, 'i'ziaereby maintaining the temperature 'and continuing the reaction throughout the mass to be comforted.

to the reaction temperature,

5. The process of making compounds of nitrogen by reacting on carbids with nitrogen at a suitable temperature, which oonsists in miXn with the carbid a carbonizabie materia to form channels or pores in the carbid mass, heating a relatively small part of the carbid mass to a. reacting tem perature, supplying nitrogen as the reaction proceeds, therebyT maintaining the tempera 

